CN106867445A - A kind of resistance to 350 DEG C of organic silicon adhesives of cold curing high intensity and application - Google Patents

A kind of resistance to 350 DEG C of organic silicon adhesives of cold curing high intensity and application Download PDF

Info

Publication number
CN106867445A
CN106867445A CN201710136171.0A CN201710136171A CN106867445A CN 106867445 A CN106867445 A CN 106867445A CN 201710136171 A CN201710136171 A CN 201710136171A CN 106867445 A CN106867445 A CN 106867445A
Authority
CN
China
Prior art keywords
parts
component
gas
resistance
organic silicon
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201710136171.0A
Other languages
Chinese (zh)
Other versions
CN106867445B (en
Inventor
吕虎
孔宪志
孙东洲
孙禹
李岳
于国良
张立颖
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Institute of Petrochemistry of Heilongjiang Academy of Sciences
Institute of Advanced Technology of Heilongjiang Academy of Sciences
Original Assignee
Institute of Petrochemistry of Heilongjiang Academy of Sciences
Institute of Advanced Technology of Heilongjiang Academy of Sciences
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Institute of Petrochemistry of Heilongjiang Academy of Sciences, Institute of Advanced Technology of Heilongjiang Academy of Sciences filed Critical Institute of Petrochemistry of Heilongjiang Academy of Sciences
Priority to CN201710136171.0A priority Critical patent/CN106867445B/en
Publication of CN106867445A publication Critical patent/CN106867445A/en
Application granted granted Critical
Publication of CN106867445B publication Critical patent/CN106867445B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/006—Additives being defined by their surface area
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Abstract

A kind of resistance to 350 DEG C of organic silicon adhesives of cold curing high intensity and application, it is related to a kind of organic silicon adhesive and application.The invention solves the problems that existing additional organosilicon adhesive high temperature bonding intensity is not high, it is impossible to meet the problem of the performance bonding requirements high such as Aero-Space.Organic silicon adhesive is made up of first component and second component；First component is prepared from by the iron oxide red of the silicones of base containing phenyl maleimide, 110 2 silicon rubber, vinyl silicone oil, the gas-phase silica, chloroplatinic acid divinyl tetramethyl disiloxane and pretreatment of pretreatment；Second component is prepared from by the silicones of base containing phenyl maleimide, 110 2 silicon rubber, vinyl silicone oil, the gas-phase silica of pretreatment, the containing hydrogen silicone oil that hydrogen content is 1.5% and titanium dioxide color masterbatch；For the bonding of the outer thermal insulation tile of aerospace craft, strain isolating pad and body titanium alloy and span composite, temperature in use is 120 DEG C~350 DEG C.

Description

A kind of resistance to 350 DEG C of organic silicon adhesives of cold curing high intensity and application
Technical field
The present invention relates to a kind of organic silicon adhesive and application.
Background technology
Additional organosilicon adhesive has high-low temperature resistant, corrosion-resistant, radiation hardness, insulating properties and good weatherability feature.Can Bonded metal, plastics, rubber, glass etc., are widely used in the fields such as Aeronautics and Astronautics, electronics, machinery, building.Domestic pair adds Shaping organic silicon adhesive has been studied, but the problem for existing is that high temperature bonding intensity is not high, is mainly used in doing fluid sealant, it is impossible to Meet the requirement of the performance bonding high such as Aero-Space.
The content of the invention
The invention solves the problems that existing additional organosilicon adhesive high temperature bonding intensity is not high, it is impossible to meet Aero-Space etc. The problem of high-performance bonding requirements, and a kind of resistance to 350 DEG C of organic silicon adhesives of cold curing high intensity and application are provided.
A kind of resistance to 350 DEG C of organic silicon adhesives of cold curing high intensity are made up of first component and second component；Described first group It is 1 to divide with the mass ratio of second component:1；
Described first component press mass fraction by 12 parts~15 parts silicones of base containing phenyl maleimide, 40 parts~45 parts 110-2 silicon rubber, 10 parts~15 parts vinyl silicone oils, the gas-phase silica of 10 parts~15 parts pretreatments, 0.015 part~0.03 part Chloroplatinic acid-divinyl tetramethyl disiloxane and the iron oxide red of 10 parts~12 parts pretreatments are prepared from；Described first group Medium vinyl silicon oil viscosity is divided to be 2000mPas~4000mPas；
The gas-phase silica pre-processed in described first component is prepared according to the following steps：5 parts are weighed by mass fraction ~7 parts of HMDSs, 100 parts of gas-phase silicas and 100 parts of viscosity are the ethene of 2000mPas~4000mPas Base silicone oil, 5 parts for then weighing~7 parts of HMDSs and 100 parts of gas-phase silicas are added to 100 parts of viscosity and are In the vinyl silicone oil of 2000mPas~4000mPas, after closed stirring 1h~2h in banbury, being warming up to temperature is 160 DEG C~180 DEG C, under conditions of being 160 DEG C~180 DEG C in temperature, stirring reaction 2h~4h after cooling, is pre-processed Gas-phase silica；The specific surface area of described gas-phase silica is 270m2/ g~300m2/g；
The iron oxide red pre-processed in described first component is prepared according to the following steps：Use quality percentage is 3% ~5% KH570 acetone solns soak 4110 iron oxide reds, are then dried in fume hood, are placed in baking oven after drying, heating It is 180 DEG C~200 DEG C to temperature, under conditions of being 180 DEG C~200 DEG C in temperature, reacts 3h~4h, cools to room temperature with the furnace, The iron oxide red for being pre-processed；
Described second component press mass fraction by 5 parts~10 parts silicones of base containing phenyl maleimide, 40 parts~50 parts 110-2 silicon rubber, 12 parts~15 parts vinyl silicone oils, 12 parts~15 parts gas-phase silica, 4 parts~6 parts hydrogen contents for pre-processing It is that 1.5% containing hydrogen silicone oil and 0.5 part of titanium dioxide color masterbatch are prepared from, described second component medium vinyl silicon oil viscosity is 2000mPas~4000mPas；The gas phase pre-processed in the gas-phase silica and first component that are pre-processed in described second component White carbon is identical.
A kind of resistance to 350 DEG C of organic silicon adhesives of cold curing high intensity are used for aerospace craft outer thermal insulation tile, strain isolating Pad is bonding with body titanium alloy and span composite, and temperature in use is -120 DEG C~350 DEG C.
The beneficial effects of the invention are as follows：The present invention passes through the surface treatment of reinforcer gas-phase silica, adds heat-resisting adding Plus the iron oxide red of agent 4110, addition phenyl maleimide base silicones, hydrogeneous silicones high etc., prepare a kind of high strength heat resistant Silicon rubber type adhesive, can be used for the bonding of aerospace craft thermally protective materials, adhesive room temperature shear strength >=7.0MPa, 350 DEG C of shear strength >=3.0MPa, intensity is substantially without decline after aging 48h.And commercially available organic silicon adhesive is bonded due to it Intensity is not high, and room temperature shear strength is only 3~5MPa, and 350 DEG C of shear strengths are less than 1MPa, and high and low temperature resistance is poor, applicable for temperature Generally -70~200 DEG C of degree, and only used as fluid sealant.
Iron oxide red is the metallic compound with oxidation-reduction effect, after adding in silicon rubber, in certain temperature Can prevent, due to the radical reaction that oxidation is produced, so as to prevent the degraded under silicon rubber high temperature, to reach raising in the range of degree The purpose of silicon rubber heat endurance.
Modified silicone resin in the adhesive is phenyl maleimide base silicones, and the structure silicones has excellent Heat resistance and adhesive property, are remarkably improved the heat-resistant fine adhesive function energy of adhesive.
The curing agent of the adhesive is a kind of containing hydrogen silicone oil high, and hydrogen content is 1.5%, by containing hydrogen silicone oil hydrogen content and first The mol ratio of all vinyl is 1.3 in component and second component:1 is matched.The catalyst for using is chloroplatinic acid-divinyl Tetramethyl disiloxane.
Specific embodiment
Specific embodiment one：Present embodiment is a kind of resistance to 350 DEG C of organic silicon adhesives of cold curing high intensity by first Component and second component are constituted；Described first component is 1 with the mass ratio of second component:1；
Described first component press mass fraction by 12 parts~15 parts silicones of base containing phenyl maleimide, 40 parts~45 parts 110-2 silicon rubber, 10 parts~15 parts vinyl silicone oils, the gas-phase silica of 10 parts~15 parts pretreatments, 0.015 part~0.03 part Chloroplatinic acid-divinyl tetramethyl disiloxane and the iron oxide red of 10 parts~12 parts pretreatments are prepared from；Described first group Medium vinyl silicon oil viscosity is divided to be 2000mPas~4000mPas；
The gas-phase silica pre-processed in described first component is prepared according to the following steps：5 parts are weighed by mass fraction ~7 parts of HMDSs, 100 parts of gas-phase silicas and 100 parts of viscosity are the ethene of 2000mPas~4000mPas Base silicone oil, 5 parts for then weighing~7 parts of HMDSs and 100 parts of gas-phase silicas are added to 100 parts of viscosity and are In the vinyl silicone oil of 2000mPas~4000mPas, after closed stirring 1h~2h in banbury, being warming up to temperature is 160 DEG C~180 DEG C, under conditions of being 160 DEG C~180 DEG C in temperature, stirring reaction 2h~4h after cooling, is pre-processed Gas-phase silica；The specific surface area of described gas-phase silica is 270m2/ g~300m2/g；
The iron oxide red pre-processed in described first component is prepared according to the following steps：Use quality percentage is 3% ~5% KH570 acetone solns soak 4110 iron oxide reds, are then dried in fume hood, are placed in baking oven after drying, heating It is 180 DEG C~200 DEG C to temperature, under conditions of being 180 DEG C~200 DEG C in temperature, reacts 3h~4h, cools to room temperature with the furnace, The iron oxide red for being pre-processed；
Described second component press mass fraction by 5 parts~10 parts silicones of base containing phenyl maleimide, 40 parts~50 parts 110-2 silicon rubber, 12 parts~15 parts vinyl silicone oils, 12 parts~15 parts gas-phase silica, 4 parts~6 parts hydrogen contents for pre-processing It is that 1.5% containing hydrogen silicone oil and 0.5 part of titanium dioxide color masterbatch are prepared from, described second component medium vinyl silicon oil viscosity is 2000mPas~4000mPas；The gas phase pre-processed in the gas-phase silica and first component that are pre-processed in described second component White carbon is identical.
The beneficial effect of present embodiment is：Present embodiment passes through the surface treatment of reinforcer gas-phase silica, adds Plus the iron oxide red of heat-resisting additive 4110, addition phenyl maleimide base silicones, hydrogeneous silicones high etc., prepare a kind of high Strength thermal resistant silicon rubber type adhesive, can be used for the bonding of aerospace craft thermally protective materials, and adhesive room temperature shear strength >= 7.0MPa, 350 DEG C of shear strength >=3.0MPa, intensity is substantially without decline after aging 48h.And commercially available organic silicon adhesive due to Its adhesive strength is not high, and room temperature shear strength is only 3~5MPa, and 350 DEG C of shear strengths are less than 1MPa, and high and low temperature resistance is poor, Applicable temperature is generally -70~200 DEG C, and is only used as fluid sealant.
Iron oxide red is the metallic compound with oxidation-reduction effect, after adding in silicon rubber, in certain temperature Can prevent, due to the radical reaction that oxidation is produced, so as to prevent the degraded under silicon rubber high temperature, to reach raising in the range of degree The purpose of silicon rubber heat endurance.
Modified silicone resin in the adhesive is phenyl maleimide base silicones, and the structure silicones has excellent Heat resistance and adhesive property, are remarkably improved the heat-resistant fine adhesive function energy of adhesive.
The curing agent of the adhesive is a kind of containing hydrogen silicone oil high, and hydrogen content is 1.5%, by containing hydrogen silicone oil hydrogen content and first The mol ratio of all vinyl is 1.3 in component and second component:1 is matched.The catalyst for using is chloroplatinic acid-divinyl Tetramethyl disiloxane.
Specific embodiment two：Present embodiment is with the difference of specific embodiment one：Described first component be by Prepared by following steps：By mass fraction weigh 12 parts~15 parts silicones of base containing phenyl maleimide, 40 parts~45 parts 110-2 silicon rubber, 10 parts~15 parts vinyl silicone oils, the gas-phase silica of 10 parts~15 parts pretreatments, 0.015 part~0.03 part Chloroplatinic acid-divinyl tetramethyl disiloxane and 10 parts~12 parts iron oxide reds of pretreatment, 12 parts for then weighing~ 15 parts of silicones of base containing phenyl maleimide, 40 parts~45 parts 110-2 silicon rubber, 10 parts~15 parts vinyl silicone oils, 10 parts ~15 parts of gas-phase silicas of pretreatment, 0.015 part~0.03 part chloroplatinic acid-divinyl tetramethyl disiloxane and 10 parts~ In 12 parts of iron oxide red input banburies of pretreatment, under conditions of being 100 DEG C~120 DEG C in temperature, closed stirring 2h~3h, After cooling, ground 2 times~3 times on three roller grinding distribution machines, obtain first component.Other are identical with specific embodiment one.
Specific embodiment three：Present embodiment is with the difference of one of specific embodiment one or two：Described second Component is prepared according to the following steps：By mass fraction weigh 5 parts~10 parts silicones of base containing phenyl maleimide, 40 parts~ 50 parts of 110-2 silicon rubber, 12 parts~15 parts vinyl silicone oils, the gas-phase silica of 12 parts~15 parts pretreatments, 4 parts~6 parts contain Hydrogen amount be 1.5% containing hydrogen silicone oil and 0.5 part of titanium dioxide color masterbatch, 5 parts for then weighing~10 parts contain benzyl maleimide Amido silicones, 40 parts~50 parts 110-2 silicon rubber, 12 parts~15 parts vinyl silicone oils, 12 parts~15 parts gas phases for pre-processing White carbon, 4 parts~6 parts hydrogen contents be 1.5% containing hydrogen silicone oil and 0.5 part of titanium dioxide color masterbatch input banbury in, in temperature Under conditions of for 100 DEG C~120 DEG C, closed stirring 2h~3h after cooling, grinds 2 times~3 times on three roller grinding distribution machines, Obtain second component.Other are identical with specific embodiment one or two.
Specific embodiment four：Present embodiment is with the difference of one of specific embodiment one to three：Described first Component press mass fraction by 15 parts of silicones of base containing phenyl maleimide, 45 parts of 110-2 silicon rubber, 13 parts of vinyl silicone oils, 13 parts of gas-phase silicas of pretreatment, 0.015 part of chloroplatinic acid-divinyl tetramethyl disiloxane and 10 parts of oxidations of pretreatment Iron oxide red is prepared from；Described first component medium vinyl silicon oil viscosity is 3200mPas.Other with specific embodiment one to Three is identical.
Specific embodiment five：Present embodiment is with the difference of one of specific embodiment one to four：Described first The gas-phase silica pre-processed in component is prepared according to the following steps：By mass fraction weigh 5 parts of HMDSs, 100 parts of gas-phase silicas and 100 parts of viscosity are the vinyl silicone oil of 3200mPas, the 5 parts of silicon of hexamethyl two that then will be weighed Azane and 100 parts of gas-phase silicas are added in the vinyl silicone oil that 100 parts of viscosity are 3200mPas, closed in banbury After stirring 1h, temperature is warming up to for 180 DEG C, under conditions of being 180 DEG C in temperature, stirring reaction 4h after cooling, is pre-processed Gas-phase silica；The specific surface area of described gas-phase silica is 290m2/g.Other and the phase of specific embodiment one to four Together.
Specific embodiment six：Present embodiment is with the difference of one of specific embodiment one to five：Described first The iron oxide red pre-processed in component is prepared according to the following steps：Use quality percentage is 5% KH570 acetone solns general 4110 iron oxide reds are soaked, and are then dried in fume hood, are placed in baking oven after drying, and are heated to temperature for 180 DEG C, are in temperature Under conditions of 180 DEG C, 4h is reacted, cool to room temperature with the furnace, the iron oxide red for being pre-processed.Other and specific embodiment one It is identical to five.
Specific embodiment seven：Present embodiment is with the difference of one of specific embodiment one to six：Described second Component presses mass fraction by 5 parts of silicones of base containing phenyl maleimide, 40 parts of 110-2 silicon rubber, 12 parts of vinyl silicone oils, 12 The gas-phase silica of part pretreatment, 6 parts of hydrogen contents are that 1.5% containing hydrogen silicone oil and 0.5 part of titanium dioxide color masterbatch are prepared from, institute The second component medium vinyl silicon oil viscosity stated is 3200mPas.Other are identical with specific embodiment one to six.
Specific embodiment eight：Present embodiment is that a kind of resistance to 350 DEG C of organic silicon adhesives of cold curing high intensity are used for The outer thermal insulation tile of aerospace craft, strain isolating pad and body titanium alloy and span composite it is bonding, temperature in use is -120 DEG C~350 DEG C.
The beneficial effect of present embodiment is：Present embodiment passes through the surface treatment of reinforcer gas-phase silica, adds Plus the iron oxide red of heat-resisting additive 4110, addition phenyl maleimide base silicones, hydrogeneous silicones high etc., prepare a kind of high Strength thermal resistant silicon rubber type adhesive, can be used for the bonding of aerospace craft thermally protective materials, and adhesive room temperature shear strength >= 7.0MPa, 350 DEG C of shear strength >=3.0MPa, intensity is substantially without decline after aging 48h.And commercially available organic silicon adhesive due to Its adhesive strength is not high, and room temperature shear strength is only 3~5MPa, and 350 DEG C of shear strengths are less than 1MPa, and high and low temperature resistance is poor, Applicable temperature is generally -70~200 DEG C, and is only used as fluid sealant.
Iron oxide red is the metallic compound with oxidation-reduction effect, after adding in silicon rubber, in certain temperature Can prevent, due to the radical reaction that oxidation is produced, so as to prevent the degraded under silicon rubber high temperature, to reach raising in the range of degree The purpose of silicon rubber heat endurance.
Modified silicone resin in the adhesive is phenyl maleimide base silicones, and the structure silicones has excellent Heat resistance and adhesive property, are remarkably improved the heat-resistant fine adhesive function energy of adhesive.
The curing agent of the adhesive is a kind of containing hydrogen silicone oil high, and hydrogen content is 1.5%, by containing hydrogen silicone oil hydrogen content and first The mol ratio of all vinyl is 1.3 in component and second component:1 is matched.The catalyst for using is chloroplatinic acid-divinyl Tetramethyl disiloxane.
Specific embodiment nine：Present embodiment is with the difference of specific embodiment eight：A kind of described cold curing The resistance to 350 DEG C of organic silicon adhesives of high intensity are specifically applied according to the following steps：By cold curing high intensity, resistance to 350 DEG C have Machine silica gel stick is extruded into treats adhesives surface, after smearing uniformly, closes up after hanging 5min~8min, is compacted with hand or rubber-surfaced roll, Then under conditions of bonding site is using gravity or vacuum pressed 0.04MPa~0.06MPa, room temperature pressurization 4h, room temperature after release 24h is placed, that is, completes a kind of application of the resistance to 350 DEG C of organic silicon adhesives of cold curing high intensity.Other and specific embodiment Eight is identical.
Using following verification experimental verifications effect of the present invention：
Embodiment one：The resistance to 350 DEG C of organic silicon adhesives of a kind of cold curing high intensity described in the present embodiment are by first component And second component composition；Described first component is 1 with the mass ratio of second component:1；
Described first component press mass fraction by 15 parts of silicones of base containing phenyl maleimide, 45 parts of 110-2 silicon rubber, 13 parts of vinyl silicone oils, the gas-phase silicas of 13 parts of pretreatments, 0.015 part of chloroplatinic acid-divinyl tetramethyl disiloxane and The iron oxide red of 10 parts of pretreatments is prepared from；Described first component medium vinyl silicon oil viscosity is 3200mPas；
The gas-phase silica pre-processed in described first component is prepared according to the following steps：5 parts are weighed by mass fraction HMDS, 100 parts of gas-phase silicas and 100 parts of viscosity are the vinyl silicone oil of 3200mPas, then will be weighed 5 parts of HMDSs and 100 parts of gas-phase silicas be added to the vinyl silicone oil that 100 parts of viscosity are 3200mPas In, after closed stirring 1h in banbury, temperature is warming up to for 180 DEG C, under conditions of being 180 DEG C in temperature, stirring reaction 4h, After cooling, the gas-phase silica for being pre-processed；The specific surface area of described gas-phase silica is 290m2/g；
The iron oxide red pre-processed in described first component is prepared according to the following steps：Use quality percentage is 5% KH570 acetone solns 4110 iron oxide reds are soaked, then dried in fume hood, be placed in baking oven after drying, be heated to temperature It is 180 DEG C to spend, and under conditions of being 180 DEG C in temperature, reacts 4h, cools to room temperature with the furnace, the iron oxide red for being pre-processed；
Described second component press mass fraction by 5 parts of silicones of base containing phenyl maleimide, 40 parts of 110-2 silicon rubber, 12 parts of vinyl silicone oils, the gas-phase silica of 12 parts of pretreatments, 6 parts of hydrogen contents be 1.5% containing hydrogen silicone oil and 0.5 part of titanium dioxide Titanium color masterbatch is prepared from, and described second component medium vinyl silicon oil viscosity is 3200mPas；Pre-processed in described second component Gas-phase silica with first component pre-process gas-phase silica it is identical.
Described first component is prepared according to the following steps：15 parts of silicon of base containing phenyl maleimide are weighed by mass fraction Resin, 45 parts of 110-2 silicon rubber, 13 parts of vinyl silicone oils, 13 parts of gas-phase silica, 0.015 part of chloroplatinic acid-diethyl for pre-processing Alkenyl tetramethyl disiloxane and 10 parts of iron oxide reds of pretreatment, the 15 parts of silicon of base containing phenyl maleimide that then will be weighed Resin, 45 parts of 110-2 silicon rubber, 13 parts of vinyl silicone oils, 13 parts of gas-phase silica, 0.015 part of chloroplatinic acid-diethyl for pre-processing It is close under conditions of being 120 DEG C in temperature in alkenyl tetramethyl disiloxane and 10 parts of iron oxide red input banburies of pretreatment Stirring 2h is closed, after cooling, is ground 3 times on three roller grinding distribution machines, obtain first component；
Described second component is prepared according to the following steps：5 parts of silicon of base containing phenyl maleimide are weighed by mass fraction Resin, 40 parts of 110-2 silicon rubber, 12 parts of vinyl silicone oils, 12 parts of gas-phase silicas for pre-processing, 6 parts of hydrogen contents are 1.5% Containing hydrogen silicone oil and 0.5 part of titanium dioxide color masterbatch, 5 parts of silicones of base containing phenyl maleimide, the 40 parts of 110-2 that then will be weighed Silicon rubber, 12 parts of vinyl silicone oils, the gas-phase silica of 12 parts of pretreatments, 6 parts of hydrogen contents are 1.5% containing hydrogen silicone oil and 0.5 In part titanium dioxide color masterbatch input banbury, under conditions of being 120 DEG C in temperature, closed stirring 2h, after cooling, in the grinding of three rollers Ground 3 times on dispersion machine, obtain second component.
First component and second component are fitted into bi-component AB ratio packing elements, piston is installed after standing 48h deaerations.Use When install that static mixing tube extrusion is usable, the packaging can save conventional bicomponent organic silicon adhesive and first weigh when in use After mix vacuum defoamation again these steps.
The resistance to 350 DEG C of organic silicon adhesives of cold curing high intensity are extruded into and treat adhesives surface, after smearing uniformly, hung Close up after 8min, be compacted with rubber-surfaced roll, then bonding site is using under conditions of vacuum pressed 0.04MPa, room temperature pressurization 4h, release Room temperature places 24h afterwards, obtains glued part；Described treats that adhesives is titanium alloy TC 4.
Glued part is performed into shear strength test, the cold curing to the present embodiment according to GB/T7124-2008 standards The resistance to 350 DEG C of organic silicon adhesives of high intensity perform 180 ° of peel strength tests according to GB/T2790-1995 standards, according to GB/ TGB/T 528-1998 standards perform tensile strength and elongation at break test, and test result is as shown in table 1：
Table 1
As shown in Table 1, adhesive room temperature shear strength >=7.0MPa, 350 DEG C of shear strength >=3.0MPa, after aging 48h Intensity is substantially without decline.And commercially available organic silicon adhesive is not high due to its adhesive strength, room temperature shear strength is only 3~ 5MPa, 350 DEG C of shear strengths are less than 1MPa, and high and low temperature resistance is poor, and Applicable temperature is generally -70~200 DEG C, and only as close Sealing is used.

Claims (9)

1. a kind of a kind of resistance to 350 DEG C of organic silicon adhesives of cold curing high intensity, it is characterised in that cold curing high intensity resistance to 350 DEG C organic silicon adhesive is made up of first component and second component；Described first component is 1 with the mass ratio of second component:1；
Described first component presses mass fraction by 12 parts~15 parts silicones of base containing phenyl maleimide, 40 parts~45 parts 110- 2 silicon rubber, 10 parts~15 parts vinyl silicone oils, 10 parts~15 parts gas-phase silica, 0.015 part~0.03 part chlorine platinum for pre-processing Acid-divinyl tetramethyl disiloxane and the iron oxide red of 10 parts~12 parts pretreatments are prepared from；In described first component Vinyl silicone oil viscosity is 2000mPas~4000mPas；
The gas-phase silica pre-processed in described first component is prepared according to the following steps：5 parts~7 parts are weighed by mass fraction HMDS, 100 parts of gas-phase silicas and 100 parts of viscosity are the vinyl silicon of 2000mPas~4000mPas Oil, 5 parts for then weighing~7 parts of HMDSs and 100 parts of gas-phase silicas are added to 100 parts of viscosity and are In the vinyl silicone oil of 2000mPas~4000mPas, after closed stirring 1h~2h in banbury, being warming up to temperature is 160 DEG C~180 DEG C, under conditions of being 160 DEG C~180 DEG C in temperature, stirring reaction 2h~4h after cooling, is pre-processed Gas-phase silica；The specific surface area of described gas-phase silica is 270m2/ g~300m2/g；
The iron oxide red pre-processed in described first component is prepared according to the following steps：Use quality percentage is 3%~5% KH570 acetone solns 4110 iron oxide reds are soaked, then dried in fume hood, be placed in baking oven after drying, be heated to temperature It is 180 DEG C~200 DEG C to spend, and under conditions of being 180 DEG C~200 DEG C in temperature, reacts 3h~4h, cools to room temperature with the furnace, is obtained The iron oxide red of pretreatment；
Described second component presses mass fraction by 5 parts~10 parts silicones of base containing phenyl maleimide, 40 parts~50 parts 110-2 Silicon rubber, 12 parts~15 parts vinyl silicone oils, 12 parts~15 parts gas-phase silicas for pre-processing, 4 parts~6 parts hydrogen contents are 1.5% containing hydrogen silicone oil and 0.5 part of titanium dioxide color masterbatch are prepared from, and described second component medium vinyl silicon oil viscosity is 2000mPas~4000mPas；The gas phase pre-processed in the gas-phase silica and first component that are pre-processed in described second component White carbon is identical.
2. resistance to 350 DEG C of organic silicon adhesives of a kind of cold curing high intensity according to claim 1, it is characterised in that described First component prepare according to the following steps：By mass fraction weigh 12 parts~15 parts silicones of base containing phenyl maleimide, 40 parts~45 parts 110-2 silicon rubber, 10 parts~15 parts vinyl silicone oils, 10 parts~15 parts gas-phase silica, 0.015 for pre-processing Part~0.03 part of chloroplatinic acid-divinyl tetramethyl disiloxane and 10 parts~12 parts iron oxide reds of pretreatment, then will claim 12 parts for taking~15 parts of silicones of base containing phenyl maleimide, 40 parts~45 parts 110-2 silicon rubber, 10 parts~15 parts vinyl Silicone oil, 10 parts~15 parts gas-phase silica, 0.015 part~0.03 part chloroplatinic acid-silica of divinyl tetramethyl two for pre-processing It is closed under conditions of being 100 DEG C~120 DEG C in temperature in alkane and 10 parts~12 parts iron oxide red input banburies of pretreatment Stirring 2h~3h, after cooling, grinds 2 times~3 times on three roller grinding distribution machines, obtains first component.
3. resistance to 350 DEG C of organic silicon adhesives of a kind of cold curing high intensity according to claim 1, it is characterised in that described Second component prepare according to the following steps：5 parts~10 parts silicones of base containing phenyl maleimide, 40 are weighed by mass fraction Part~50 parts of 110-2 silicon rubber, 12 parts~15 parts vinyl silicone oils, 12 parts~15 parts gas-phase silica, 4 parts~6 for pre-processing Part hydrogen content be 1.5% containing hydrogen silicone oil and 0.5 part of titanium dioxide color masterbatch, 5 parts for then weighing~10 parts of Malaysias containing phenyl Imide silicones, 40 parts~50 parts 110-2 silicon rubber, 12 parts~15 parts vinyl silicone oils, 12 parts~15 parts pretreatments Gas-phase silica, 4 parts~6 parts hydrogen contents be 1.5% containing hydrogen silicone oil and 0.5 part of titanium dioxide color masterbatch input banbury in, Temperature is under conditions of 100 DEG C~120 DEG C, closed stirring 2h~3h after cooling, grinds 2 times~3 on three roller grinding distribution machines It is secondary, obtain second component.
4. resistance to 350 DEG C of organic silicon adhesives of a kind of cold curing high intensity according to claim 1, it is characterised in that described First component press mass fraction by 15 parts of silicones of base containing phenyl maleimide, 45 parts of 110-2 silicon rubber, 13 parts of vinyl silicon What oil, 13 parts of gas-phase silicas for pre-processing, 0.015 part of chloroplatinic acid-divinyl tetramethyl disiloxane and 10 parts were pre-processed Iron oxide red is prepared from；Described first component medium vinyl silicon oil viscosity is 3200mPas.
5. resistance to 350 DEG C of organic silicon adhesives of a kind of cold curing high intensity according to claim 1, it is characterised in that described First component in pre-process gas-phase silica prepare according to the following steps：5 parts of silicon nitrogen of hexamethyl two are weighed by mass fraction Alkane, 100 parts of gas-phase silicas and 100 parts of viscosity are the vinyl silicone oil of 3200mPas, the 5 parts of hexamethyls two that then will be weighed Silazane and 100 parts of gas-phase silicas are added in the vinyl silicone oil that 100 parts of viscosity are 3200mPas, close in banbury After closing stirring 1h, temperature is warming up to for 180 DEG C, under conditions of being 180 DEG C in temperature, stirring reaction 4h after cooling, obtains pre- place The gas-phase silica of reason；The specific surface area of described gas-phase silica is 290m2/g。
6. resistance to 350 DEG C of organic silicon adhesives of a kind of cold curing high intensity according to claim 1, it is characterised in that described First component in pre-process iron oxide red prepare according to the following steps：Use quality percentage be 5% KH570 acetone it is molten Liquid soaks 4110 iron oxide reds, is then dried in fume hood, is placed in baking oven after drying, and temperature is heated to for 180 DEG C, in temperature Spend under conditions of 180 DEG C, to react 4h, cool to room temperature with the furnace, the iron oxide red for being pre-processed.
7. resistance to 350 DEG C of organic silicon adhesives of a kind of cold curing high intensity according to claim 1, it is characterised in that described Second component press mass fraction by 5 parts of silicones of base containing phenyl maleimide, 40 parts of 110-2 silicon rubber, 12 parts of vinyl silicon Oil, the gas-phase silica of 12 parts of pretreatments, the containing hydrogen silicone oil that 6 parts of hydrogen contents are 1.5% and 0.5 part of titanium dioxide color masterbatch prepare and Into described second component medium vinyl silicon oil viscosity is 3200mPas.
8. a kind of application of the resistance to 350 DEG C of organic silicon adhesives of cold curing high intensity as claimed in claim 1, it is characterised in that A kind of resistance to 350 DEG C of organic silicon adhesives of cold curing high intensity are used for aerospace craft outer thermal insulation tile, strain isolating pad and body The bonding of titanium alloy and span composite, temperature in use is -120 DEG C~350 DEG C.
9. a kind of application of the resistance to 350 DEG C of organic silicon adhesives of cold curing high intensity according to claim 8, its feature exists Specifically applied according to the following steps in a kind of described resistance to 350 DEG C of organic silicon adhesives of cold curing high intensity：By room The temperature solidification resistance to 350 DEG C of organic silicon adhesives of high intensity are extruded into treats adhesives surface, after smearing uniformly, after hanging 5min~8min Close up, be compacted with hand or rubber-surfaced roll, under conditions of then bonding site is using gravity or vacuum pressed 0.04MPa~0.06MPa, room Temperature pressurization 4h, room temperature places 24h after release, that is, complete a kind of application of the resistance to 350 DEG C of organic silicon adhesives of cold curing high intensity.
CN201710136171.0A 2017-03-08 2017-03-08 Application of room-temperature-cured high-strength 350-DEG C-resistant organic silicon adhesive Expired - Fee Related CN106867445B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710136171.0A CN106867445B (en) 2017-03-08 2017-03-08 Application of room-temperature-cured high-strength 350-DEG C-resistant organic silicon adhesive

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710136171.0A CN106867445B (en) 2017-03-08 2017-03-08 Application of room-temperature-cured high-strength 350-DEG C-resistant organic silicon adhesive

Publications (2)

Publication Number Publication Date
CN106867445A true CN106867445A (en) 2017-06-20
CN106867445B CN106867445B (en) 2020-06-09

Family

ID=59171203

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710136171.0A Expired - Fee Related CN106867445B (en) 2017-03-08 2017-03-08 Application of room-temperature-cured high-strength 350-DEG C-resistant organic silicon adhesive

Country Status (1)

Country Link
CN (1) CN106867445B (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107674633A (en) * 2017-11-02 2018-02-09 嘉善天胶装饰材料有限公司 A kind of mirror bottom dedicated weather-proof glue and preparation method thereof
CN110041877A (en) * 2019-03-14 2019-07-23 湖北航聚科技有限公司 A kind of good bonding agent of thermal matching and preparation method thereof
CN111320965A (en) * 2020-03-27 2020-06-23 无锡市百合花胶粘剂厂有限公司 High-temperature-resistant adhesive, and preparation method and application thereof
CN115449330A (en) * 2022-08-25 2022-12-09 黑龙江省科学院石油化学研究院 Bi-component high-performance polyurethane sealant and preparation method and application thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104262632A (en) * 2014-10-14 2015-01-07 黑龙江省科学院石油化学研究院 Phenylmaleimide based silicone resin, preparation method thereof, silicone adhesive prepared by phenylmaleimide based silicone resin and application of silicone adhesive
CN104861923A (en) * 2015-05-27 2015-08-26 湖北三江航天江北机械工程有限公司 Silastic material having high bonding strength with metal and preparation method of silastic material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104262632A (en) * 2014-10-14 2015-01-07 黑龙江省科学院石油化学研究院 Phenylmaleimide based silicone resin, preparation method thereof, silicone adhesive prepared by phenylmaleimide based silicone resin and application of silicone adhesive
CN104861923A (en) * 2015-05-27 2015-08-26 湖北三江航天江北机械工程有限公司 Silastic material having high bonding strength with metal and preparation method of silastic material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
张玉龙: "《粘接技术手册》", 31 August 2001, 中国轻工业出版社 *
曲艳斌等: "耐热阻燃硅橡胶的研制", 《有机硅材料》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107674633A (en) * 2017-11-02 2018-02-09 嘉善天胶装饰材料有限公司 A kind of mirror bottom dedicated weather-proof glue and preparation method thereof
CN110041877A (en) * 2019-03-14 2019-07-23 湖北航聚科技有限公司 A kind of good bonding agent of thermal matching and preparation method thereof
CN111320965A (en) * 2020-03-27 2020-06-23 无锡市百合花胶粘剂厂有限公司 High-temperature-resistant adhesive, and preparation method and application thereof
CN115449330A (en) * 2022-08-25 2022-12-09 黑龙江省科学院石油化学研究院 Bi-component high-performance polyurethane sealant and preparation method and application thereof
CN115449330B (en) * 2022-08-25 2023-08-08 黑龙江省科学院石油化学研究院 Double-component high-performance polyurethane sealant and preparation method and application thereof

Also Published As

Publication number Publication date
CN106867445B (en) 2020-06-09

Similar Documents

Publication Publication Date Title
CN106867445A (en) A kind of resistance to 350 DEG C of organic silicon adhesives of cold curing high intensity and application
CN104974711B (en) High-temperature resistance organic silicon adhesive
CN103030976B (en) Single-component heat-curing liquid silicone rubber and preparation method thereof
Yoo et al. Investigation of curing kinetics of various cycloaliphatic epoxy resins using dynamic thermal analysis
CN101768363A (en) Method for preparing addition highly heat-conducting room temperature-curing silicon rubber
CN105315958A (en) Addition heat-conducting self-adhesive silicone rubber and preparation method thereof
CN103694711B (en) A kind of oil-resistant fluorosilicone rubber and preparation method thereof
CN105441020B (en) A kind of fluorine silicone encapsulant for aircraft integral tank sealing
CN101812233A (en) Bicomponent addition type room curing silicon rubber and preparation method thereof
CN101570680A (en) High-temperature resistant and expediting setting dealcoholized type room temperature vulcanized silicone rubber adhesive and preparation method thereof
CN107177345A (en) A kind of heat conduction Silica hydrogel and preparation method
CN109401724A (en) A kind of solar energy encapsulation one-component electric silica gel and preparation method thereof
CN105331116A (en) One-component heating-cured liquid silicone rubber and preparation method thereof
CN108219474A (en) A kind of glass-fiber-fabric enhances heat-conducting silica gel sheet
Kaddami et al. Silica‐filled poly (HEMA) from hema/grafted SiO2 nanoparticles: Polymerization kinetics and rheological changes
Wang et al. High-temperature bonding performance of modified heat-resistant adhesive for ceramic connection
CN106753214A (en) A kind of resistant to elevated temperatures silicone sealants
CN107987788A (en) A kind of primary coat type of exempting from is used for ketoxime removing type single-component silicon rubber of the water-fast bonding of hydrophilic aluminium foil and preparation method thereof
CN109370511B (en) A kind of silicone sealants and preparation method thereof
Zhai et al. Curing kinetics study by FTIR spectroscopy and properties analysis of methyl silicone resin membrane
CN105754350A (en) High-heat-conductivity gel sheet and preparation method thereof
CN105368330A (en) Alpha-cyanoacrylate heat-conducting glue and preparation method thereof
CN104725879A (en) Ablation-resistant organosilicon composite, and preparation method and application thereof
CN106147676A (en) A kind of preparation method of silicon carbide whisker silica filled organopolysiloxane resin high temperature adhesive
Li et al. Polyborosilazane preceramic as matrix resin of high temperature adhesive for graphite bonding

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20200609

CF01 Termination of patent right due to non-payment of annual fee